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采用分散液液微萃取-高效液相色谱-二极管阵列检测法测定废水中的 11 种优先污染物酚类。

Determination of 11 priority pollutant phenols in wastewater using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-diode-array detection.

机构信息

Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.

出版信息

Anal Bioanal Chem. 2010 Apr;396(7):2685-93. doi: 10.1007/s00216-010-3496-z. Epub 2010 Feb 13.

DOI:10.1007/s00216-010-3496-z
PMID:20155249
Abstract

Dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography-diode-array detection was applied for the extraction and determination of 11 priority pollutant phenols in wastewater samples. The analytes were extracted from a 5-mL sample solution using a mixture of carbon disulfide as the extraction solvent and acetone as the dispersive solvent. After extraction, solvent exchange was carried out by evaporating the solvent and then reconstituting the residue in a mixture of methanol-water (30:70). The influences of different experimental dispersive liquid-liquid microextraction parameters such as extraction solvent type, dispersive solvent type, extraction and dispersive solvent volume, salt addition, and pH were studied. Under optimal conditions, namely pH 2, 165-microL extraction solvent volume, 2.50-mL dispersive solvent volume, and no salt addition, enrichment factors and limits of detection ranged over 30-373 and 0.01-1.3 microg/L, respectively. The relative standard deviation for spiked wastewater samples at 10 microg/L of each phenol ranged between 4.3 and 19.3% (n = 5). The relative recovery for wastewater samples at a spiked level of 10 microg/L varied from 65.5 to 108.3%.

摘要

分散液液微萃取结合高效液相色谱-二极管阵列检测法用于萃取和测定废水中的 11 种优先污染物苯酚。将分析物从 5mL 样品溶液中用二硫化碳作为萃取溶剂和丙酮作为分散溶剂的混合物萃取。萃取后,通过蒸发溶剂并将残留物重新溶解在甲醇-水(30:70)混合物中进行溶剂交换。研究了不同实验分散液液微萃取参数,如萃取溶剂类型、分散溶剂类型、萃取和分散溶剂体积、加盐和 pH 的影响。在最佳条件下,即 pH 2、萃取溶剂体积 165μL、分散溶剂体积 2.50mL 且不加盐,富集因子和检测限范围分别为 30-373 和 0.01-1.3μg/L。在 10μg/L 的每种苯酚的废水样品加标时,相对标准偏差在 4.3-19.3%(n=5)之间。在加标水平为 10μg/L 的废水样品中的相对回收率在 65.5-108.3%之间变化。

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